CN116178987A - 一种可用于对纺织品进行染色的蓝色系染料及其染色方法 - Google Patents
一种可用于对纺织品进行染色的蓝色系染料及其染色方法 Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/41—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using basic dyes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B62/00—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves
- C09B62/44—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group not directly attached to a heterocyclic ring
- C09B62/62—Reactive dyes, i.e. dyes which form covalent bonds with the substrates or which polymerise with themselves with the reactive group not directly attached to a heterocyclic ring the reactive group being an ethylenimino or N—acylated ethylenimino group or a —CO—NH—CH2—CH2—X group, wherein X is a halogen atom, a quaternary ammonium group or O—acyl and acyl is derived from an organic or inorganic acid, or a beta—substituted ethylamine group
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/02—Material containing basic nitrogen
- D06P3/04—Material containing basic nitrogen containing amide groups
- D06P3/14—Wool
- D06P3/18—Wool using basic dyes
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/6016—Natural or regenerated cellulose using basic dyes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
本发明提供一种可用于对纺织品进行染色的蓝色系染料及其染色方法,其中,该染料是在吩噻嗪结构基础上进行衍生,引入活性卤素;该类染料可以在中性或碱性条件下通过形成化学键的方式对织物进行染色,该染料的染色方法为浸染法。采用该染料以及染色方法对纤维织物进行染色,染色后的产品外观均呈现出鲜亮的蓝色,并表现出优异的耐干/湿摩擦牢度和耐皂洗牢度,甚至对产品汽蒸定形长达30min时,其色调深度并无肉眼可见的明显变化。
Description
技术领域
本发明属于纺织染色领域,具体涉及一种可用于对纺织品进行染色的蓝色系染料及其染色方法。
背景技术
染料工业在我国化工行业领域中具有举足轻重的地位,2017年我国的染料年产量就达到了99万吨,并且仍在逐年递增,我国也持续占据着世界染料年产量第一的位置。近年来,伴随着人民生活水平的逐步提高和生活美学多元化的需求,人们已经不满足于单纯对染料数量上的追求,而是更加希望在染料类型上有所创新。在诸多类型的染料中,市场对具有能在水溶液中电离出色素阳离子性能的碱性染料(阳离子染料)特别是蓝色系染料的需求变得愈发旺盛,预计2022年碱性染料的市场规模将超过1000亿元人民币。然而当前常用的碱性染料如碱性蓝、碱性蓝6B、碱性品蓝、碱性艳蓝BO、碱性湖蓝B等普遍存在耐光色牢度和耐洗色牢度差的问题,这些问题严重制约了碱性染料特别是蓝色系碱性染料的应用,使其无法满足市场上对碱性染料的需求。因此,当前亟需开发性能更加优异的蓝色系碱性染料以满足市场的需求。
经典的吩噻嗪染料亚甲基蓝(MB)由于其价格低廉、容易获取,常常被用于织物染色或其它工业原料。其本身带正电荷,能够与纤维素纤维、蛋白质纤维发生静电吸附作用,从而上染到织物上,同时亚甲基蓝本身结构简单、相对分子质量低(319.852,阴离子为Cl-),与纤维间的范德华力也十分微弱,由此导致亚甲基蓝对于纤维的染色耐洗色牢度低,并且只能用于染浅色。针对上述问题,我们研究发现,在吩噻嗪结构基础上进行衍生,引入活性卤素可以使染料以化学共价键的方式与织物纤维进行结合,从而提高染料的上染率与耐洗色牢度。利用该类型染料对织物进行染色目前尚无相关报道。
发明内容
本发明的目的在与提供一种可用于对纺织品进行染色的蓝色系染料,该类染料可以在中性或碱性条件下通过形成化学键的方式对织物进行染色。
为实现上述目的,本发明提供以下技术方案:
一种可用于对纺织品进行染色的蓝色系染料,该蓝色系染料具有式Ι所示的结构:
其中:
(3)R1、R2、R3、R4各自独立地或均为F、Cl、Br、I等卤素原子;
(4)该结构在使用时的抗阴离子为氟离子、氯离子、溴离子、碘离子、硫酸根离子、高氯酸根离子、六氟磷酸根离子等负离子。
优选地,该纺织品的种类包括但不限于蛋白质纤维与纤维素纤维。
优选地,该类化合物在中性或者碱性条件下,通过与纤维形成共价键的方式,达到染色的目的;其中,在反应中,R1、R2、R3、R4至少一个与纤维织物表面上裸露的活性基团反应形成共价键。
优选地,所述活性基团包括羟基、氨基、巯基。
优选地,所述共价键包括醚键、硫醚键、碳氮键。
本发明的另一个目的是提供含有上述结构的蓝色系染料与纺织品的染色方法,该染色方法是浸染法。
优选地,该方法包括以下步骤:
(1)配制染液:将染料、中性盐、表面活性剂和去离子水混合,加入pH调节剂,调节染液pH为6.5-7.5,其中染液中,染料量为0.8%-5%o.w.f,中性盐用量为1.5-2.5g/L,表面活性剂包含分散剂和渗透剂,分散剂的质量分数为0.5%-20%(优选10%),渗透剂的质量分数为0.5%-1.5%(优选1%);
(2)将待染色的纤维织物与配置好的染液按照浴比1:5~1:30混合,于50-60℃始染30min,然后以4℃/min的速率升温至75-90℃染色60min,接着以2.5℃/min的速率降温至40℃,依次水洗三次、2g/L的皂洗液皂洗15min,最后烘干即可。
优选地,所述中性盐为硫酸钠或氯化钠,所述pH调节剂为乙酸铵、碳酸钠或碳酸氢钠,
优选地,所述渗透剂为脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚中的一种或两种;所述分散剂为无机分散剂或有机分散剂,其中,无机分散剂可以选硅酸盐类(例如水玻璃)和碱金属磷酸盐类(例如三聚磷酸钠、六偏磷酸钠和焦磷酸钠等)。有机分散剂包括十二烷基硫酸钠、纤维素衍生物、聚丙烯酰胺、瓜尔胶等。
本发明的有益效果:
本发明提供的一种可用于对纺织品进行染色的蓝色系染料,该类染料可以在中性或碱性条件下通过形成化学键的方式对织物进行染色,染色采用浸染方式,染色后的产品均表现出优异的耐干湿摩擦牢度、耐皂洗牢度的鲜亮的蓝色,甚至对产品汽蒸定形长达30min时,其色调深度并无肉眼可见的明显变化。
附图说明
图1该染料与纤维织物的染色机理示意图;
图2为该染料的染色工艺流程简图;
图3左上为MB干摩擦后的标准摩擦布,右上为MB湿摩擦后的标准摩擦布;左下为C1干摩擦后的标准摩擦布,右下为C1湿摩擦后的标准摩擦布;
图4使用MB染料染色布样皂洗前后图片(左为皂洗前,右为皂洗后);
图5使用C1染料染色布样皂洗前后图片(左为皂洗前,右为皂洗后);
图6为本发明染料采用不同染色方法的染色效果对比图。
具体实施方式:
下面结合实施例对本发明进行具体描述。
实施例1制备下列结构的染料(如表1所示):
表1
该染料的详细制备方法,步骤如下:
(1)起始化合物为吩噻嗪(1g),溶于二氯甲烷溶液中,低温下(优选<0℃)分批加入碘单质(4g)。加入完毕后,室温下搅拌反应,TLC跟踪反应结束。将体系过滤,弃去滤液,得到四碘代吩噻嗪4.5g。
(2)将四碘代吩噻嗪(1g,1当量)溶于甲醇中,共制备四份;然后低温下分别加入对应的胺(C1:双(2-氯乙基)胺;C2:双(2-溴乙基)胺;C3:双(2-碘乙基)胺;C4:双(2-氟乙基)胺;),其中胺的用量为5-10倍当量,优选10倍当量;滴加完毕后TLC跟踪反应结束。反应结束后蒸干溶剂,使用二氯甲烷溶解、过滤,滤液使用柱层析纯化(流动相为甲醇和二氯甲烷,两者的比例在1/10到1/20之间,优选1:15)分别得到对应目标产物C1-C4。
此时目标化合物的抗阴离子不单一,可以为反应体系中存在的阴离子,如氟离子、氯离子、溴离子、碘离子、硫酸根离子、高氯酸根离子、六氟磷酸根离子等负离子。如果想使产物的抗阴离子单一,可以通过如下方式进行离子交换。将1g(1倍当量)产物溶解于甲醇中,加入不同类型的盐(如氯化钠、六氟磷酸钠等10当量),搅拌反应过夜,随后将体系倒入二氯甲烷溶液中,二次水多次洗液后将有机相浓缩蒸干即可使产物的抗阴离子与加入的盐一致。
实施例2采用实施例1所得染料(C1-C4)分别对纤维织物(羊毛)进行染色,染色方法如下(参照图2所示):
(1)配制染液:
将染料、中性盐(硫酸钠)、表面活性剂(分散剂和渗透剂)和去离子水混合,加入pH调节剂(乙酸铵),调节染液pH为6.5-7.5,其中染液中,染料量为1%o.w.f,硫酸钠用量为1.5g/L;分散剂(三聚磷酸钠)的质量分数为10%;渗透剂(脂肪醇聚氧乙烯醚)的质量分数为1.5%;
(2)将待染色的纤维织物(白色羊毛布料5g)与配置好的染液按照浴比1:20混合,于50-60℃始染30min,然后以4℃/min的速率升温至75-90℃染色60min,接着以2.5℃/min的速率降温至40℃,依次水洗三次、2g/L的皂洗液皂洗15min,最后烘干即可。
本发明的染料的染色机理,参照图1所示。
本发明所得染料(C1-C4)对织物进行染色后的性能评价如表2所示(参照GB251):
表2
实施例3采用实施例1所得染料(C1-C4)对纤维织物(羊毛)进行染色,染色方法参照实施例2所示,与实施例2不同的是,染液中,染料量为5%o.w.f,硫酸钠用量为2.0g/L,分散剂(三聚磷酸钠)的质量分数为20%;渗透剂(脂肪醇聚氧乙烯醚)的质量分数为0.8%。
实施例4采用实施例1所得染料(任选一种)对纤维织物(棉)进行染色,染色方法参照实施例2所示,与实施例2不同的是,染液中染料量为0.8%o.w.f,中性盐(氯化钠)用量为1.8g/L,分散剂(聚丙烯酰胺)的质量分数为0.5%;渗透剂(烷基酚聚氧乙烯醚)的质量分数为0.5%,纤维织物与染液的浴比1:30混合。
实施例5采用实施例1所得染料(任选一种)对纤维织物(棉)进行染色,染色方法参照实施例2所示,与实施例2不同的是,染液中染料量为2%o.w.f,中性盐(氯化钠)用量为2.5g/L,分散剂(水玻璃)的质量分数为3%;渗透剂(烷基酚聚氧乙烯醚)的质量分数为1%,纤维织物与染液的浴比1:5混合。
试验发现,采用实施例1和实施例5所描述的染色方法,所得到的产品均表现出优异的耐干湿摩擦牢度、耐皂洗牢度的鲜亮的蓝色,甚至对产品汽蒸定形长达30min时,其色调深度并无肉眼可见的明显变化。
对比试验1
选用下面两种原料,采用实施例2的染色方法对同一种纤维织物进行染色。
染色后的织物相关性能测试数据如下:
(1)上染率:MB:10-20%;C1:>90%。
(2)耐干湿摩擦牢度(通过标准沾色卡比较,参照GB251),结果如图3和表3所示。
表3
耐皂洗牢度的测试
相关实验参数:温度:50℃、时间:45min、钢珠数量:0、碳酸钠:0(此处是否撰写有误)、浴比:1:50;皂洗液:每升三级水中5g皂片,即5g/L;
耐皂洗牢度执行标准:GB/T3921 B
结果如图4和图5所示,通过灰色样卡的比较(GB251)得到耐皂洗牢度等级:MB:1级;C1:5级。
对比实验2
采用原料C1以轧染的方式对织物进行染色。
染液:去离子水:25ml;染料:20g/L;尿素:20g/L;表面活性剂:1%;
碱液:NaOH:5g/L;体积:110mL;
工艺流程:1)浸轧染液(两浸两轧,带液率100%);2)预烘(100℃,1min);3)浸轧碱液(两浸两轧,带液率100%);4)焙烘(100℃,1min);5)汽蒸(100℃,5min);6)皂洗(1.5g/L,15min);7)水洗。
最后获得的布样如图6所示,染色的颜色非常浅,并且染色不均匀;表明现有的轧染工艺不如本发明提供的浸染方法效果好。
应当指出的是,具体实施方式只是本发明比较有代表性的例子,显然本发明的技术方案不限于上述实施例,还可以有很多变形。本领域的普通技术人员,以本发明所明确公开的或根据文件的书面描述毫无异议的得到的,均应认为是本专利所要保护的范围。
Claims (9)
2.权利要求1所述的蓝色系染料在纺织品染色中的应用,该纺织品的种类包括但不限于蛋白质纤维与纤维素纤维。
3.如权利要求2所述的蓝色系染料在纺织品上的应用,其特征在于,该类化合物在中性或者碱性条件下,通过与纤维形成共价键的方式,达到染色的目的;其中,在反应中,R1、R2、R3、R4至少一个与纤维织物表面上裸露的活性基团反应形成共价键。
4.如权利要求3所述的蓝色系染料在纺织品上的应用,其特征在于,所述活性基团包括羟基、氨基、巯基等。
5.如权利要求3所述的蓝色系染料在纺织品上的应用,其特征在于,所述共价键包括醚键、硫醚键、碳氮键等。
6.一种如权利要求1-5任一所述的蓝色系染料与纺织品的染色方法,其特征在于,该染色方法是浸染法。
7.如权利要求6所述的染色方法,其特征在于,该方法包括以下步骤:
(1)配制染液:将染料、中性盐、表面活性剂和去离子水混合,加入pH调节剂,调节染液pH为6.5-7.5,其中染液中染料量为0.8%-5%o.w.f,中性盐用量为1.5-2.5g/L,表面活性剂包括分散剂和渗透剂;其中,分散剂占染液的质量分数为0.5%-20%(优选10%),渗透剂占染液的质量分数为0.5%-1.5%(优选1%);
(2)将待染色的纤维织物与配置好的染液按照浴比1:5~1:30混合,于50-60℃始染30min,然后以4℃/min的速率升温至75-90℃染色60min,接着以2.5℃/min的速率降温至40℃,依次水洗三次、2g/L的皂洗液皂洗15min,最后烘干即可。
8.根据权利要求7所述的染色方法,其特征在于,所述中性盐为硫酸钠或氯化钠,所述pH调节剂为乙酸铵、碳酸钠或碳酸氢钠等。
9.根据权利要求7所述的染色方法,其特征在于,所述渗透剂为脂肪醇聚氧乙烯醚、烷基酚聚氧乙烯醚中的一种或两种;所述分散剂为无机分散剂或有机分散剂。
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CSABA, GYORGY等: "《A new antitumor agent; a phenazathionium mustard salt》", 《NEOPLASMA》, vol. 15, no. 4, 31 December 1968 (1968-12-31), pages 443 - 5 * |
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